eCrystals - Southampton

Coles, Simon J.

Hursthouse, Michael B.

Kilic, A.

Davies, David B.

Table 1.  Crystal data and structure refinement for 2009src0404.
Identification code 	2009src0404
Empirical formula 	C12 H24 Cl8 N6 O4 P6
Formula weight 	785.79
Temperature 	120(2) K
Wavelength 	0.71073 Å
Crystal system 	Triclinic
Space group 	P-1
Unit cell dimensions	a = 10.1145(4) Å	a= 72.775(3)º.
	b = 10.9859(5) Å	b= 72.933(3)º.
	c = 15.0878(6) Å	g = 73.224(3)º.
Volume	1492.97(11) Å3
Z	2
Density (calculated)	1.748 Mg/m3
Absorption coefficient	1.110 mm-1
F(000)	792
Crystal size	0.26 x 0.09 x 0.02 mm3
Theta range for data collection	3.10 to 27.50º.
Index ranges	-13<=h<=13, -14<=k<=14, -19<=l<=19
Reflections collected	34049
Independent reflections	6837 [R(int) = 0.1098]
Completeness to theta = 27.50º	99.5 % 
Absorption correction	Semi-empirical from equivalents
Max. and min. transmission	0.9781 and 0.7612
Refinement method	Full-matrix least-squares on F2
Data / restraints / parameters	6837 / 0 / 325
Goodness-of-fit on F2	1.033
Final R indices [I>2sigma(I)]	R1 = 0.0592, wR2 = 0.1106
R indices (all data)	R1 = 0.1117, wR2 = 0.1288
Largest diff. peak and hole	0.549 and -0.508 e.Å-3
Chirality: P1=R, P3=S, P4=S, P6=R, P4b=R, P6b=S.
P1-P2 = 2.740, P2-P3 = 2.740, P1-P3 = 2.768, Max Dev=0.102(P2).
P4-P5 = 2.750, P5-P6 = 2.742, P4-P6 = 2.768, Max Dev=0.037(P5)
Table 2.  Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (Å2x 103)
for 2009src0404.  U(eq) is defined as one third of the trace of the orthogonalized Uij tensor.
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	x	y	z	U(eq)
________________________________________________________________________________
C(5)	303(5)	2571(4)	3132(3)	26(1)
C(1)	240(4)	1719(4)	7139(3)	25(1)
C(2)	-238(5)	1055(4)	6583(3)	23(1)
C(3)	36(5)	-426(4)	6942(3)	23(1)
C(4)	-394(5)	-1132(4)	6384(3)	22(1)
C(6)	674(4)	3348(5)	3657(3)	28(1)
C(7)	5695(4)	1263(4)	2243(3)	25(1)
C(8)	5461(4)	393(4)	1716(3)	23(1)
C(9)	3949(4)	212(4)	1995(3)	27(1)
C(10)	3744(4)	-692(4)	1473(3)	23(1)
C(11)	4474(5)	-2112(4)	1776(3)	27(1)
C(12)	5614(5)	2980(5)	-1191(3)	30(1)
N(1)	4235(3)	1918(3)	6063(2)	21(1)
N(2)	4457(4)	2668(3)	4151(2)	21(1)
N(3)	1919(3)	3279(3)	5349(2)	23(1)
N(4)	9255(3)	2409(4)	964(2)	24(1)
N(5)	9264(3)	3251(4)	-927(2)	24(1)
N(6)	6775(3)	3237(4)	404(2)	24(1)
O(1)	1812(3)	1458(3)	6906(2)	21(1)
O(2)	2184(3)	2841(3)	3696(2)	20(1)
O(3)	7173(3)	1393(3)	1906(2)	24(1)
O(4)	7131(3)	2901(3)	-1288(2)	22(1)
P(1)	2584(1)	2547(1)	6243(1)	18(1)
P(2)	5189(1)	2143(1)	5019(1)	19(1)
P(3)	2829(1)	3358(1)	4293(1)	19(1)
P(4)	7584(1)	2667(1)	1243(1)	19(1)
P(5)	10099(1)	2622(1)	-106(1)	22(1)
P(6)	7583(1)	3568(1)	-676(1)	19(1)
Cl(1)	2177(1)	3839(1)	7050(1)	26(1)
Cl(2)	6605(1)	480(1)	4867(1)	30(1)
Cl(3)	6485(1)	3296(1)	4901(1)	32(1)
Cl(4)	2661(1)	5265(1)	3634(1)	33(1)
Cl(5)	6869(1)	3917(1)	2110(1)	26(1)
Cl(6)	11543(1)	3643(1)	-288(1)	33(1)
Cl(7)	11369(1)	920(1)	-344(1)	41(1)
Cl(8)	6896(1)	5484(1)	-1218(1)	30(1)
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Table 3.   Bond lengths [Å] and angles [º] for 2009src0404.
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C(5)-C(6) 	1.503(6)
C(5)-C(4)#1 	1.521(6)
C(1)-O(1) 	1.484(5)
C(1)-C(2) 	1.508(6)
C(2)-C(3) 	1.524(6)
C(3)-C(4) 	1.515(6)
C(4)-C(5)#1 	1.521(6)
C(6)-O(2) 	1.479(5)
C(7)-O(3) 	1.466(5)
C(7)-C(8) 	1.513(6)
C(8)-C(9) 	1.519(6)
C(9)-C(10) 	1.525(6)
C(10)-C(11) 	1.516(6)
C(11)-C(12)#2 	1.514(6)
C(12)-O(4) 	1.477(5)
C(12)-C(11)#2 	1.514(6)
N(1)-P(2) 	1.578(3)
N(1)-P(1) 	1.587(3)
N(2)-P(2) 	1.571(4)
N(2)-P(3) 	1.581(4)
N(3)-P(1) 	1.580(4)
N(3)-P(3) 	1.581(3)
N(4)-P(5) 	1.573(3)
N(4)-P(4) 	1.578(3)
N(5)-P(5) 	1.579(4)
N(5)-P(6) 	1.585(3)
N(6)-P(6) 	1.578(3)
N(6)-P(4) 	1.583(4)
O(1)-P(1) 	1.554(3)
O(2)-P(3) 	1.556(3)
O(3)-P(4) 	1.548(3)
O(4)-P(6) 	1.562(3)
P(1)-Cl(1) 	2.0145(15)
P(2)-Cl(2) 	1.9968(15)
P(2)-Cl(3) 	2.0107(15)
P(3)-Cl(4) 	2.0160(15)
P(4)-Cl(5) 	2.0137(15)
P(5)-Cl(6) 	1.9989(16)
P(5)-Cl(7) 	2.0031(17)
P(6)-Cl(8) 	2.0131(15)

C(6)-C(5)-C(4)#1	115.1(4)
O(1)-C(1)-C(2)	109.7(3)
C(1)-C(2)-C(3)	113.3(4)
C(4)-C(3)-C(2)	114.8(4)
C(3)-C(4)-C(5)#1	111.9(3)
O(2)-C(6)-C(5)	108.5(3)
O(3)-C(7)-C(8)	108.7(3)
C(7)-C(8)-C(9)	113.3(3)
C(8)-C(9)-C(10)	112.5(3)
C(11)-C(10)-C(9)	114.2(4)
C(12)#2-C(11)-C(10)	113.9(4)
O(4)-C(12)-C(11)#2	107.6(3)
P(2)-N(1)-P(1)	120.0(2)
P(2)-N(2)-P(3)	120.8(2)
P(1)-N(3)-P(3)	122.3(2)
P(5)-N(4)-P(4)	121.6(2)
P(5)-N(5)-P(6)	120.2(2)
P(6)-N(6)-P(4)	122.2(2)
C(1)-O(1)-P(1)	119.9(3)
C(6)-O(2)-P(3)	120.1(3)
C(7)-O(3)-P(4)	121.9(3)
C(12)-O(4)-P(6)	120.1(3)
O(1)-P(1)-N(3)	111.65(18)
O(1)-P(1)-N(1)	107.13(17)
N(3)-P(1)-N(1)	118.25(18)
O(1)-P(1)-Cl(1)	103.85(12)
N(3)-P(1)-Cl(1)	107.35(14)
N(1)-P(1)-Cl(1)	107.61(14)
N(2)-P(2)-N(1)	119.04(18)
N(2)-P(2)-Cl(2)	108.93(14)
N(1)-P(2)-Cl(2)	108.40(14)
N(2)-P(2)-Cl(3)	109.31(14)
N(1)-P(2)-Cl(3)	109.23(15)
Cl(2)-P(2)-Cl(3)	100.29(7)
O(2)-P(3)-N(3)	112.07(17)
O(2)-P(3)-N(2)	107.39(17)
N(3)-P(3)-N(2)	117.49(18)
O(2)-P(3)-Cl(4)	103.02(12)
N(3)-P(3)-Cl(4)	107.51(14)
N(2)-P(3)-Cl(4)	108.33(14)
O(3)-P(4)-N(4)	107.56(18)
O(3)-P(4)-N(6)	112.14(18)
N(4)-P(4)-N(6)	117.51(18)
O(3)-P(4)-Cl(5)	102.81(12)
N(4)-P(4)-Cl(5)	107.91(15)
N(6)-P(4)-Cl(5)	107.84(15)
N(4)-P(5)-N(5)	119.60(18)
N(4)-P(5)-Cl(6)	108.75(15)
N(5)-P(5)-Cl(6)	109.09(14)
N(4)-P(5)-Cl(7)	109.15(15)
N(5)-P(5)-Cl(7)	108.20(15)
Cl(6)-P(5)-Cl(7)	100.33(7)
O(4)-P(6)-N(6)	111.26(18)
O(4)-P(6)-N(5)	106.84(18)
N(6)-P(6)-N(5)	118.63(19)
O(4)-P(6)-Cl(8)	102.88(12)
N(6)-P(6)-Cl(8)	108.09(15)
N(5)-P(6)-Cl(8)	107.97(14)



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Symmetry transformations used to generate equivalent atoms: 
#1 -x,-y,-z+1    #2 -x+1,-y,-z 


Table 4.   Anisotropic displacement parameters (Å2x 103)for 2009src0404.  The anisotropic
displacement factor exponent takes the form: -2p2[ h2a*2U11 + ... + 2 h k a* b* U12 ]
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	U11	U22	U33	U23	U13	U12
______________________________________________________________________________
C(5)	23(2) 	26(2)	30(2) 	-4(2)	-12(2) 	-4(2)
C(1)	19(2) 	28(3)	26(2) 	-9(2)	4(2) 	-10(2)
C(2)	23(2) 	24(2)	20(2) 	-4(2)	-4(2) 	-7(2)
C(3)	26(2) 	25(2)	17(2) 	-2(2)	-6(2) 	-9(2)
C(4)	23(2) 	26(2)	18(2) 	-4(2)	-6(2) 	-7(2)
C(6)	21(2) 	31(3)	37(3) 	-13(2)	-14(2) 	-3(2)
C(7)	23(2) 	27(2)	24(2) 	-4(2)	-2(2) 	-10(2)
C(8)	26(2) 	28(2)	15(2) 	-8(2)	-1(2) 	-9(2)
C(9)	21(2) 	30(3)	35(3) 	-9(2)	-6(2) 	-10(2)
C(10)	18(2) 	28(2)	24(2) 	-5(2)	-2(2) 	-10(2)
C(11)	26(2) 	27(3)	32(3) 	-2(2)	-15(2) 	-8(2)
C(12)	21(2) 	36(3)	41(3) 	-16(2)	-13(2) 	-5(2)
N(1)	19(2) 	27(2)	17(2) 	-3(2)	-5(2) 	-4(2)
N(2)	22(2) 	31(2)	13(2) 	-7(2)	-3(1) 	-9(2)
N(3)	19(2) 	30(2)	19(2) 	-5(2)	-6(2) 	-2(2)
N(4)	18(2) 	34(2)	19(2) 	-1(2)	-9(2) 	-4(2)
N(5)	17(2) 	34(2)	20(2) 	-8(2)	0(2) 	-7(2)
N(6)	13(2) 	38(2)	18(2) 	-3(2)	-4(2) 	-4(2)
O(1)	21(2) 	21(2)	20(2) 	-3(1)	-3(1) 	-10(1)
O(2)	18(2) 	21(2)	25(2) 	-7(1)	-11(1) 	-3(1)
O(3)	22(2) 	26(2)	26(2) 	-2(1)	-6(1) 	-11(1)
O(4)	20(2) 	25(2)	24(2) 	-8(1)	-8(1) 	-7(1)
P(1)	18(1) 	19(1)	17(1) 	-4(1)	-4(1) 	-4(1)
P(2)	16(1) 	25(1)	20(1) 	-8(1)	-3(1) 	-7(1)
P(3)	22(1) 	20(1)	16(1) 	-2(1)	-6(1) 	-8(1)
P(4)	16(1) 	24(1)	16(1) 	-2(1)	-4(1) 	-6(1)
P(5)	16(1) 	28(1)	23(1) 	-8(1)	-4(1) 	-7(1)
P(6)	18(1) 	25(1)	16(1) 	-4(1)	-5(1) 	-6(1)
Cl(1)	30(1) 	25(1)	28(1) 	-12(1)	-5(1) 	-7(1)
Cl(2)	21(1) 	31(1)	39(1) 	-15(1)	-5(1) 	-2(1)
Cl(3)	29(1) 	37(1)	37(1) 	-12(1)	-7(1) 	-17(1)
Cl(4)	51(1) 	23(1)	30(1) 	1(1)	-18(1) 	-15(1)
Cl(5)	29(1) 	25(1)	25(1) 	-8(1)	-4(1) 	-9(1)
Cl(6)	26(1) 	47(1)	34(1) 	-13(1)	-5(1) 	-18(1)
Cl(7)	31(1) 	37(1)	54(1) 	-21(1)	-7(1) 	4(1)
Cl(8)	39(1) 	24(1)	32(1) 	-3(1)	-16(1) 	-8(1)
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University of Southampton

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2009src0404

2009src1135

C~15~H~13~N~3~O~2~

2008src1280

2009src0082

N-(2-methylphenyl)acetamide

N-(3-bromophenyl)acetamide

2009src0297

2008src1083

2009src0464

Data sources:

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